Title: Standardising sodium hydroxide solution

Aim: 1. To prepare a standard solution of 0.15 M 250 mL of hydrochloric acid, HCl. 2. To determine the concentration of sodium hydroxide, NaOH, solution.

Independent variable: Concentration of sodium hydroxide, NaOH, solution. It can be determined by using calculation method after being titrated with HCl solution.

Dependant variable Average titre value of hydrochloric acid, HCl, solution. By dividing three concordant titre value of HCl solution that is used to titrate NaOH solution.

Constant variable: 1. 2. 3. 4. Volume of sodium hydroxide, NaOH, solution, that is 25.0mL Concentration of hydrochloric acid, HCl, which is 0.15 M. Type of indicator used which is methyl orange. Number of drops of methyl orange indicator that is fixed to 3 drops.

Introduction Titration, also known as titrimetry is a common laboratory technique of quantitative chemical analysis used to determine the concentration of unknown by measuring the volume of unknown required to react with volume of identified analyte. There are two types of titration, one is Acid-base titration and the other one is redox titration. An acid-base titration is the determination of the concentration of an acid or base by exactly neutralizing the acid or base with an acid or base of known concentration. Redox titration (also called oxidation-reduction titration) is a type of titration based on a redox reaction between the analyte and titrant. A pH indicator is an organic substance that is added in small amounts to a solution so that the pH (acidity or basicity) of the solution can be determined visually. In titration, an indicator is used to signal the endpoint of a neutralization process. For example, in an experiment using methyl red as indicator, when sodium hydroxide solution is titrated toward

HCl solution, the endpoint of the neutralization the moment the indicator change to permanent yellow colour. A standard solution is a solution with accurately known concentration. A standard solution can be prepared by two ways. One is by dissolving the primary standard (a compound which is stable, of high purity, highly soluble in water and of a high molar mass to allow for accurate weighing) and another is by diluting a stock solution. Once a solution has been standardized in one direction, it may be used as a standard solution for the subsequent reaction.

Procedure: 1. 0.5 M of HCl stock solution that was prepared by the lab assistant was obtained by using a 100 mL beaker. 2. Unknown concentration of NaOH solution was obtained by using a 200 mL beaker. 3. Before using the pipette to transfer HCl, rinse the pipette with HCl first. Followed by pipetting 75 mL of HCl stock solution into the volumetric flask. However, volumetric pipette can only hold a maximum volume of 25 mL, therefore 3 times pipetting must be allowed in order to get the exact volume of HCl. 4. Deionised water was added into the volumetric flask until the bottom meniscus touches the calibration mark. The flask was stoppered and the mixing was completed by repeating inversion. 5. The burette was rinsed with deionised water, followed by rinsing with 10 mL of standard HCl solution that was prepared. The burette was hold almost horizontal and was rotated to ensure the rinsing solution covers all the inside of burette. 6. 0.15 M HCl solution was poured into the burette with the aid of filter funnel. The burette was gently tapped if there were air bubbles trapped in the column. 7. 5 mL of NaOH was drawn into the pipette for rinsing. The pipette was held almost horizontal to ensure the rinsing covered all of the inside. NaOH was drawn into the pipette past the 25 mL mark and then drained. 8. 25.0 mL of NaOH solution was pipetted into the conical flask. The pipette was held vertically and the tip of pipette touches the inner wall of conical flask. 10 seconds of draining time was allowed after the last drop was delivered. The inner wall of the conical flask was rinsed with deionised water to make sure the NaOH solution is well mixed. 3 drops of methyl orange indicator was added into the conical flask. Methyl orange indicator: 0.04% (w/v) methyl orange (sodium salt) 9. The initial reading of burette was recorded before titration. The flask was swirled gently after each addition of HCl solution to mix the solution. The end point was reached when the solution turned to an orange red colour. The final reading of burette was recorded. 10. Titration process was repeated until three concordant titre values were obtained. The conical flask was rinsed with deionised water between titration.

Result and Calculation

Part A: Preparation of 0.150 mol/L of HCl stock solution from 0.500 mol/L HCl stock solution. 1. Volume of 0.500 mol/L HCl stock solution C1V1 = C2V2 V1 = = = 75.00 mL

2. Concentration of diluted HCl prepared C1V1 = C2V2 C2 = =

= 0.15 M

Part B: To determine the concentration of NaOH

Volume of Experiment NaOH (mL) 1 2 3 25.0 25.0 25.0

Burette Reading (mL) Final 20.00 20.00 19.90 Initial 0.00 0.00 0.00

Volume of HCl (mL) 20.00 20.00 19.90

Concordant titre =

mL

= 19.9667 mL

= 19.97 mL (3 sf) Concentration of NaOH solution: NaOH + HCl NaCl + H2O

n(HCl) = C x V n(HCl) = 0.15 x 19.97 x 10-3 n(HCl) = 2.9955 x 10-3 moles n(HCl) = 3.0 x 10-3 moles

=1x = 1 x 3.0 x 10-3 moles = 3.0 x 10-3 moles (2 sf)

Discussion: 1. Pattern of the result It is found out that the concentration of diluted HCl prepared from 75.00 mL of 0.500 mol/L HCl stock solution was 0.150 mol/L by using calculation method. The endpoint of titration was reached when the colour of methyl orange indicator changes from yellow to orange-red. The final reading of the burette was recorded.

2. Accuracy and precision of the results

Precision The concordant of titre values obtained were 20.0 mL, 20.0 mL, and 19.90 mL. The average concordant titre value was 19.97 mL.This data shows high precision as 3 concordant titre values were obtained in the experiment.

Accuracy By referring to the calculation, the concentration of NaOH solution obtained was 0.120 mol/L. Therefore the data obtained was slightly inaccurate compared to the actual concentration of NaOH solution, which is 0.125 mol/L.

3. Correct handling of volumetric glassware i. Burette

The burette was filled with diluted HCl solution and the barrel was rotated horizontally so that the remaining deionised water does not dilute the HCl solution when rinsing. Besides,HCl solution was drained through the tap of the burette so that deionised water left will not dilute the HCl solution. When filling up the burette, the level of HCl solution was adjusted until the bottom meniscus of HCl solution coincide with the calibration mark so that accurate amount of HCl solution had been transferred. Air bubbles were removed if it is found as the air bubbles occupy space and thus affecting the total volume of HCl solution in the burette. The tip of the burette was filled with HCl solution because the HCl solution in the tip of the burette is also considered as the initial burette reading. The HCl solution in the burette was delivered slowly using left hand turn and right hand swirl method. The process of titration was continued until the endpoint was reached whereby the indicator changes colour from yellow to orange-red. Volumetric pipette The pipette was rinsed with deionised water, followed by rinsing with NaOH solution so that the NaOH solution will not be diluted by the deionised water remaining inside the pipette. When filling up the volumetric pipette, use a pipette filler to draw in the NaOH solution until well above the calibration mark so that the amount of NaOH solution is accurate as possible. The pipette was ensured in vertical position and no air bubbles were trapped in the pipette as these air bubbles occupy space in the pipette which will reduce the volume of NaOH solution pipetted. The tip of the pipette touches the inner wall of the conical flask to ensure correct amount of NaOH solution was delivered. 10 seconds of draining time was allowed after the last drop was delivered and do not blow out or forced out the remaining NaOH solution at the tip of the volumetric pipette. If it is blown out, the concentration of NaOH solution will increase.

ii.

iii.

iv.

Volumetric flask The volumetric flask was rinsed with deionised water to make sure that it is clean. Do not heat or use hot water in the volumetric flask as this would change the calibration mark of the volumetric flask. Conical flask The conical flask was rinsed with deionised water so that it is clean.

4. Rinsing and its effect on the titre value i. Burette

If the burette is only rinsed with deionised water, the concentration of the HCl solution will dilute by the remaining water and thus more HCl solution will be needed to titrate the NaOH solution. Therefore, titre value increases.

ii.

Volumetric pipette If the pipette is only rinsed with deionised water, the concentration of NaOH solution will be lower as the NaOH solution is diluted by the remaining water in the pipette. So, less volume of HCl solution will be needed to neutralize the NaOH solution. Thus, the titre value decreases

iii.

Volumetric flask If the volumetric flask is rinsed with HCl solution instead of deionised water, the concentration of the HCl solution will increase and thus the titre value will decrease.

5. Sources of errors i.
Systematic error Uncalibrated pipette causes the volume of NaOH to be slightly higher than the actual volume which will increase the concentration of NaOH solution and decrease the titre value. So it will increase the scatter and reduce accuracy. Concentration of HCl solution that was wrongly prepared causes the titre value to be higher or lower, so it will be difficult to obtained 3 concordant titre value and reduced the accuracy. Contaminated NaOH solution will cause the concentration of NaOH solution to be slightly higher or lower which leads to the inaccuracy of titre value. Fast flowing of HCl solution into NaOH solution, causing insufficient time to react between HCl and NaOH solution which will lowers the titre value and finally lowering the average titre value.

ii.

Random error Excess drops of methyl orange indicator into the NaOH solution will increase the titre value; therefore increase the volume of HCl solution. The burette is not filled properly in a sense that air bubbles were trapped will cause the initial reading of the burette to be wrongly recorded and thus it causes the volume of HCl solution to be lower, so it increase the scatter and reduces precision value.

6. Improvement to the design of the experiment. i. Close the volumetric flask which contains HCl solution with stopper after
every use to prevent the contamination of HCl solution.

ii.

Change the methyl red indicator with pH meter so that the equivalence point can be known and no excess titre value added into the conical flask. It is done by placing the electrodes of pH meter into the NaOH solution and obtained the reading from the pH meter.

iii.

Add HCl solution drop by drop into the conical flask to minimize the excess amount of titre value added to the conical flask.

7. The importance of number of samples and repeating the experiment.

It is necessary to increase the number of samples by replicating the experiment to get concordant titre to reduce the effect of random error and to improve precision of the result. It is also important to repeating the experiment by using different method such as by adding the amount of titre value into the conical flask containing NaOH solution to reduce the effect of systematic error and check the accuracy of the data.

8. Safety assessment i. ii. iii.

HCl solution is corrosive, it will cause blindness upon eye contact, so it is necessary to wear goggle when handling acid Burette, pipette, volumetric flask and conical flask are fragile; it needs to be handling with care. NaOH solution is hazardous in case of skin or eye contact. It causes severe burn to our skin and inflammation upon eye contact. Therefore NaOH solution must be handling with care in order to prevent irritation to our skin or eye.

9. Collaboration
In this experiment, my role is to perform the titration and my partners role is to prepare a standard HCl solution by diluting the HCL stock solution. While my partner is preparing the HCl solution, I was rinsing the burette, pipette and the conical flask with deionised water. After the preparation standard HCl solution was done, my partner helped me to set up the titration by filling up the burette with HCl solution. As for me, I prepared the NaOH solution by pipetting into the conical flask, followed by adding 3 drops of methyl orange indicator. After each time of titration, my partner helped me to take the reading in the burette as the end point of titration was reached when the colour changes from yellow to orange-red. We were able to obtained 3 concordant titre value at the end of the experiment. We should spend more time on finding ways to strengthen our teamwork because the current experiment that we managed to carry out did not worked out well as there were once I over-titrating the NaOH solution where the colour changes from yellow to pink.

10. Conclusion
For the concordant titre values we obtained, it shows that 19.97 mL of HCl solution with a concentration of 0.15 mol/L was used to neutralise the 25 mL of NaOH solution. After obtaining the concordant titre value, we were able to calculate the concentration of NaOH solution. Based on the calculation obtained, the experimental value of concentration of NaOH was 0.120 mol/L.

From the data obtained, it shows high precision as 3 concordant titre values were obtained from the experiment, which is 20.00 mL, 20.00 mL and 19.90 mL. Besides that, the experimental result of concentration of NaOH solution was less accurate as the actual concentration of NaOH solution was 0.125 mol/L.

However, the aim of the experiment was achieved as 0.15 M of standard HCl solution was prepared in the experiment. Lastly, the concentration of NaOH solution can also be determined by calculation method, using the concordant titre value in the experiment.